CN101559984A - Preparation method of superparamagnetic Fe3O4 nano-particles - Google Patents
Preparation method of superparamagnetic Fe3O4 nano-particles Download PDFInfo
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- CN101559984A CN101559984A CNA2009100153665A CN200910015366A CN101559984A CN 101559984 A CN101559984 A CN 101559984A CN A2009100153665 A CNA2009100153665 A CN A2009100153665A CN 200910015366 A CN200910015366 A CN 200910015366A CN 101559984 A CN101559984 A CN 101559984A
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Abstract
The invention relates to a preparation method of superparamagnetic Fe3O4 nano-particles, belonging to the field of inorganic nano material preparation. The method is characterized in that the method adopts nontoxic glycerin, arginine, water and ferric iron as raw materials to synthesize high-quality superparamagnetic nano Fe3O4. The method features reasonable design of technical proposal, simple operation, easy control of reaction, good repeatability, no pollution and good safety. The prepared Fe3O4 nano-particles have high saturated magnetic intensity and tiny coercivity, can be conveniently combined with antibodies, are excellent super-magnetic nano materials and can be widely applied to the field of biomedicines.
Description
Technical field
The present invention relates to a kind of preparation method of superparamagnetic Fe 3 O 4 nano-particles, belong to field of inorganic nano-material preparation.
Background technology
Ferriferrous oxide nano-particle is used widely in the field in magnetic fluid, catalysis, target administration, immobilized enzyme, Magnetic resonance imaging, data storage, environmental improvement owing to its excellent character.In most of biomedical applications, the ferriferrous oxide nano-particle that diameter is positioned at the 10-20 nano-scale range shows best character, and each ferriferrous oxide nano-particle becomes a single magnetic domain, shows superparamagnetism more than critical temperature.Single magnetic particle has very large fixed magnetic moment, just as a very large paramagnetic atom, externally-applied magnetic field there is quick response and negligible magnetic remanence (remanent magnetization) is arranged and coercivity (making the specific magnetising moment drop to zero needed externally-applied magnetic field) (Angew.Chem.Int.Ed.2007,46,1222).These character make superparamagnetic Fe 3 O 4 nano-particles can avoid the risk of reuniting in vivo, thereby in biomedical sector is used very remarkable advantages are arranged.
In the synthetic method of existing ferriferrous oxide nano-particle, the requirement that method synthetic nanoparticles such as coprecipitation method, microemulsion method, ultrasonic radiation method do not reach biomedical applications because of the dispersiveness of its non-constant and degree of crystallinity.The synthetic method of high-quality superparamagnetic Fe 3 O 4 nano-particles mainly is the organometallics that the high boiling organic solvent interior heat is decomposed iron, this method great majority iron carbonyl ([Fe (CO)
5]), praseodynium iron ([Fe-(acac)
3]), cupferronate ([Fe (Cup)
3]) and organometallic compound such as iron oleate do source of iron, the organometallics of these iron and the high boiling organic solvent of using have very large toxicity and very expensive, and can only be distributed in the non-polar solvent before the product long time without surface modification, be not suitable for biomedical sector.Therefore we select nontoxic glycerine for use, arginine, and water and trivalent iron salt have synthesized high-quality super paramagnetic nano Z 250 as raw material, and can easily combine with biomacromolecule.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of preparation method of superparamagnetic Fe 3 O 4 nano-particles.
A kind of preparation method of superparamagnetic Fe 3 O 4 nano-particles, step is as follows:
1) take by weighing anhydrous trivalent iron salt of 0.1-1.0g and 0.5-5.0g arginine and be dissolved in the 5-20mL water, add the 5-20mL polyvalent alcohol then, ultrasonic or stirring mixes it;
2) the uniform mixing liquid that step (1) is obtained places in the stainless steel cauldron of inner liner polytetrafluoroethylene, the capping still, under 150 ℃～250 ℃ constant temperatures, react 2～36h, after reaction finishes, naturally cool to room temperature, with washing under the products therefrom room temperature three times, centrifugation or magnetic separate then, product is distributed to makes nano ferriferrous oxide suspension in the polar solvent.
Described trivalent iron salt is a kind of in iron(ic) chloride, ferric sulfate, the iron acetate.
Described polyvalent alcohol is a kind of in ethylene glycol, the glycerine.
Described step 2) reaction is meant reactor is placed in the baking oven of energy accurate temperature controlling under the constant temperature in.
The thing of product adopts Bruker D8 x-ray diffractometer with Cu-K alpha-ray (wavelength X=1.54178 mutually by X-ray diffraction spectra (XRD) test
) for diffraction light sources product is made X light diffracting analysis.
The pattern of product shows by transmission electron microscope photo (TEM), adopts Hitachi model H-700 transmission electron microscope, and acceleration voltage is 100kV.
The magnetic of product is at room temperature tested with MicroMag 2900 magnetic testers.
The present invention utilizes nontoxic raw material to synthesize high-quality superparamagnetic Fe 3 O 4 nano-particles, and reasonable in design, simple to operate, easy control of reaction, good reproducibility, pollution-free, security good.Prepared ferriferrous oxide nano-particle has very high magnetic saturation intensity and minimum coercive force, can be easily and antibodies, and be a kind of well super magnetic Nano material, can be widely used in biomedical sector.
Description of drawings
Fig. 1 is the X-ray diffraction spectra (XRD) of the ferriferrous oxide nano-particle of embodiment 1 preparation.
Fig. 2 is the transmission electron microscope photo (TEM) of the ferriferrous oxide nano-particle of embodiment 1 preparation.
Fig. 3 is that the magnetic hysteresis under the ferriferrous oxide nano-particle room temperature of embodiment 1 preparation is returned curve.
Embodiment
The present invention will be further described below in conjunction with embodiment, but be not limited thereto.
The thing of the superparamagnetic Fe 3 O 4 nano-particles of following examples preparation adopts Bruker D8 x-ray diffractometer with Cu-K alpha-ray (wavelength X=1.54178 mutually by X-ray diffraction spectra (XRD) test
) for diffraction light sources product is made X light diffracting analysis; The pattern of product shows by transmission electron microscope photo (TEM), adopts Hitachi modelH-700 transmission electron microscope, and acceleration voltage is 100kV; The magnetic of product is at room temperature tested with MicroMag 2900 magnetic testers.
Embodiment 1: the preparation method of superparamagnetic Fe 3 O 4 nano-particles, and step is as follows:
1) takes by weighing the anhydrous FeCl of 0.3g
3Be dissolved in the 10mL water with the 2.0g arginine, add 10mL glycerine then, ultrasonic it is mixed;
2) the uniform mixing liquid that step (1) is obtained places in the stainless steel cauldron of inner liner polytetrafluoroethylene, the capping still, under 200 ℃ of constant temperatures, react 6h, after reaction finishes, naturally cool to room temperature, with washing under the products therefrom room temperature three times, magnetic separates then, product is distributed to makes nano ferriferrous oxide suspension in the water.Reaction is meant reactor is placed in the baking oven of energy accurate temperature controlling under the above-mentioned constant temperature.
Fig. 1 is the ferriferrous oxide nano-particle X-ray diffraction spectra of preparation.Wherein spike can index be the diffraction peak of inverse spinel structure Z 250, its lattice parameter a=8.389
Be in close proximity to the numerical value a=8.396 that standard card (JCPDS card no.19-0629) is reported
Stronger diffraction peak shows that the crystallinity of prepared ferriferrous oxide nano-particle is better relatively.
Fig. 2 is the ferriferrous oxide nano-particle TEM photo of preparation, and as can be seen from the figure product is made up of the homogeneous nanoparticle of mean diameter 13 nanometers.
Fig. 3 returns curve for the magnetic hysteresis of the ferriferrous oxide nano-particle of preparation, and as can be seen from the figure product has superparamagnetism.
Embodiment 2:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 2h under 200 ℃ of constant temperatures.
Embodiment 3:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 12h under 200 ℃ of constant temperatures.
Embodiment 4:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 36h under 200 ℃ of constant temperatures.
Embodiment 5:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 6h under 250 ℃ of constant temperatures.
Embodiment 6:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 6h under 180 ℃ of constant temperatures.
Embodiment 7:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 6h under 150 ℃ of constant temperatures.
Embodiment 8:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to react 36h under 150 ℃ of constant temperatures.
Embodiment 9:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with the anhydrous FeCl of 0.1g
3, the 0.5g arginine.
Embodiment 10:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with the anhydrous FeCl of 0.1g
3, the 3.0g arginine.
Embodiment 11:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to use 0.5g FeCl
3, the 5.0g arginine.
Embodiment 12:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to use 1.0g FeCl
3, the 0.5g arginine.
Embodiment 13:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is that behind the adding 10mL glycerine, stirring mixes it.
Embodiment 14:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with 5mL water and 5mL glycerine.
Embodiment 15:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with 15mL water and 5mL glycerine.
Embodiment 16:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with 5mL water and 15mL glycerine.
Embodiment 17:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is, with 20mL water and 20mL glycerine.
Embodiment 18:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with example 1, and difference is to use centrifugation.
Embodiment 19:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with embodiment 1, and difference is to use 10mL ethylene glycol.
Embodiment 20:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with embodiment 1, and difference is to replace iron(ic) chloride with 0.3g ferric sulfate.
Embodiment 21:
The preparation method of superparamagnetic Fe 3 O 4 nano-particles, step are with embodiment 1, and difference is to use the 0.3g iron acetate.
Claims (4)
1, a kind of preparation method of ferriferrous oxide nano-particle, step is as follows:
1) take by weighing 0.1-1.0g trivalent iron salt and 0.5-5.0g arginine and be dissolved in the 5-20mL water, add the 5-20mL polyvalent alcohol then, ultrasonic or stirring mixes it;
2) the uniform mixing liquid that step (1) is obtained places in the stainless steel cauldron of inner liner polytetrafluoroethylene, the capping still, under 150 ℃～250 ℃ constant temperatures, react 2～36h, after reaction finishes, naturally cool to room temperature, with washing under the products therefrom room temperature three times, centrifugation or magnetic separate then, product is distributed to makes nano ferriferrous oxide suspension in the polar solvent.
2, the preparation method of a kind of ferriferrous oxide nano-particle as claimed in claim 1 is characterized in that, described trivalent iron salt is a kind of in iron(ic) chloride, ferric sulfate, the iron acetate.
3, the preparation method of a kind of ferriferrous oxide nano-particle as claimed in claim 1 is characterized in that, described polyvalent alcohol is a kind of in ethylene glycol, the glycerine.
4, the preparation method of a kind of ferriferrous oxide nano-particle as claimed in claim 1 is characterized in that, reaction is meant reactor is placed in the baking oven of energy accurate temperature controlling under the constant temperature described in the step (2).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805026A (en) * | 2010-03-12 | 2010-08-18 | 南京大学 | Method for preparing spherical super-paramagnetic ferroferric oxide nano-clusters |
| CN101863517A (en) * | 2010-05-27 | 2010-10-20 | 复旦大学 | Preparation method of mesopore-controllable magnetic microsphere |
| CN106348348A (en) * | 2016-07-28 | 2017-01-25 | 北京林业大学 | Functionalized porous ferroferric oxide nano material for efficiently collecting oil-bearing algae and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674478A (en) * | 2012-06-04 | 2012-09-19 | 复旦大学 | Method for preparing Fe3O4 magnetic nanocrystalline clusters based on microwave technology |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101172664A (en) * | 2006-11-01 | 2008-05-07 | 中国民航大学 | Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain |
| CN101409125A (en) * | 2008-08-06 | 2009-04-15 | 徐州诺特化工有限公司 | Method for preparing specificity function magneto fluid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805026A (en) * | 2010-03-12 | 2010-08-18 | 南京大学 | Method for preparing spherical super-paramagnetic ferroferric oxide nano-clusters |
| CN101863517A (en) * | 2010-05-27 | 2010-10-20 | 复旦大学 | Preparation method of mesopore-controllable magnetic microsphere |
| CN101863517B (en) * | 2010-05-27 | 2012-02-08 | 复旦大学 | Preparation method of mesopore-controllable magnetic microsphere |
| CN106348348A (en) * | 2016-07-28 | 2017-01-25 | 北京林业大学 | Functionalized porous ferroferric oxide nano material for efficiently collecting oil-bearing algae and preparation method thereof |
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